Performance of a polymer electrolyte alcohol electrosynthesis cell (PEAEC) using a glycolic acid (GC)/oxalic acid (OX) redox couple was enhanced via the multiscale approach, i.e., increase of reaction rate on an anode by employing nanometer-scale (nanoscale) IrO 2 catalysts and increase of selectivity for GC production via optimization of cell structures, i.e., a millimeter-scale approach. We prepared nanoscale IrO 2 anode catalyst, which is mixture of IrO 2 nanoparticles (d = 3.7 ± 1.8 nm) and their agglomerates (d < 200 nm). The linear sweep voltammetry measurement for water oxidation revealed that the nanoscale IrO 2 catalyst deposited on a porous carbon paper reduces overpotential for water oxidation by 196 mV from that obtained with an anode composed of commercial microscale IrO 2 grans. Furthermore, application of the nanoscale IrO 2 catalyst on porous titanium paper not only improved durability but also doubly enhanced water oxidation performance. We examined various PEAEC architectures composed of the nanoscale IrO 2 applied Ti anode. Both nanometer- and millimeter-scale approaches realized the best PEAEC performance for GC production, i.e., 59.4% of energy conversion efficiency with 97.1% of Faradaic efficiency for the GC production at 1.8 V and 98.9% of conversion for 3 M OX, which is an almost saturated aqueous solution at operating temperature of the PEAEC (60 °C).
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